Sample Pretreatment Technology Based On Noval Carbon Foam And Multi-functional Organic Polymer Nanospheres Materials And Its Application

Sample pretreatment is an important step in analytical procedures.Many solid phase adsorption-based sample pretreatment technology,such as solid-phase extraction(SPE),solid-phase microextraction(SPME),dispersive solid-phase extraction(d-SPE),micro-solid-phase extraction(p-SPE),and stir bar sorptive extraction(SBSE)have been widely used in the detection of environmental pollutants in recent years.High performance adsorption materials can ensure the efficiency and speed of pretreatment so as to achieve the accuracy of analytical results.Due to the designability of materials,many materials have been designed and used for the analysis of organic pollutants in environmental samples,such as graphene,carbon nanotubes,metal-organic framework materials(MOFs),molecular imprinted polymers(MIPs),etc.Although these materials show good adsorption properties,the synthesis of these materials is time-consuming and expensive,even using organic toxic reagents.Due to the existence of these problems,the adsorption performance of the material is limited to a certain extent.In this study,two kinds of materials,carbon foam(CF)and microporous organic polymer nanospheres(xPCMS-g-PDMAEMA)were designed and used in the pretreatment of environmental samples,and two methods for detecting environmental pollutants were developed.CF was used for solid phase microextraction analysis of polybrominated diphenyl ethers(PBDEs)in environmental water samples,and xPCMS-g-PDMAEMA was used for dispersive solid-phase extraction analysis of fluoroquinolones(FQs)in environmental water and biological samples,establishing a new methods for determination of PBDEs and FQs compounds in environmental samples,respectively.The developed methods were applied to analyse environmental samples in different locations for validating methods,and this paper discusses the possible adsorption mechanism combined with the results of materials for the characterization.The main results of this paper are as follows:1.The raw materials used in CF synthesis are cheap,clean and environment-friend materials.Through a series of reactions,carbon foam with porosity and huge specific surface area is finally formed.By optimizing a series of experimental parameters,CFs solid-phase microextraction of trace PBDEs in water,combined with GC-MS./MS analysis,an efficient and rapid analysis method was established.The good recoveries ranged 71.8%to 114.4%was obtained,and limits of detection and quantitation of six PBDEs were 0.25-2.0 ng/L and 1.0-5.0 ng/L,respectively.Intre-day and inter-day repeatability were 4.8%-6.3%and 5.8%-7.8%respectively,meeting the standard of analysis.2.xPCMS-g-PDMAEMA was good water-dispersive and dual responsive to temperature and pH,for which the size of material particle can be adjustedt by changing the temperature and pH value,thus improving the adsorption performance of the material.Below the low critical solution temperature(LCST)or acidic condition,PDMAEMA chains were swollen and the material particle size increases,which was conducive to the contact between sorbent and targets in solution,as a results,improving the adsorption performance.When the temperature was higher than LCST or the solution was under alkaline condition,PDMAEMA chains showed shrinking and adsorption capacity of sorbent decreased.In combination with LC-MS/MS detection of compounds,xPCMS-g-PDMAEMA was used for dispersive solid-phase extraction of FQs in water,and by optimizing a series of experimental parameters,such as temperature,pH value,extraction time,etc.,an efficient method for the analysis of trace FQs in environmental samples was established.The recoveries of environmental samples were 71.0%-108.5%,and limits of detection and quantitation of five FQs were 5-6.7 and 12-20 ng/L,respectively.The linear range was 0.2-10?g/L with correlation coefficients(r)>0.99.Intre-day and inter-day repeatability were 6.3-9.6%and 11.5-12.9%,respectively,meeting the standard of analysis.Based on the new adsorption materials,the method of analysing trace organic pollutants in the environment was established in this paper,which is of great significance to the analysis of trace organic pollutants in the environment,and has a good application prospect.